WO1996003446A1 - Poudre fine de fluororesine fondue, de masse moleculaire elevee, article moule obtenu et leur procede de production - Google Patents

Poudre fine de fluororesine fondue, de masse moleculaire elevee, article moule obtenu et leur procede de production Download PDF

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Publication number
WO1996003446A1
WO1996003446A1 PCT/JP1995/001423 JP9501423W WO9603446A1 WO 1996003446 A1 WO1996003446 A1 WO 1996003446A1 JP 9501423 W JP9501423 W JP 9501423W WO 9603446 A1 WO9603446 A1 WO 9603446A1
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Prior art keywords
molecular weight
molten resin
molding
copolymer
fine powder
Prior art date
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PCT/JP1995/001423
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English (en)
Japanese (ja)
Inventor
Katsuhide Otani
Kiyohiko Ihara
Original Assignee
Daikin Industries, Ltd.
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Application filed by Daikin Industries, Ltd. filed Critical Daikin Industries, Ltd.
Priority to DE69530927T priority Critical patent/DE69530927T2/de
Priority to US08/765,454 priority patent/US6365243B1/en
Priority to EP95925140A priority patent/EP0773244B1/fr
Publication of WO1996003446A1 publication Critical patent/WO1996003446A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F214/18—Monomers containing fluorine
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00—Post-polymerisation treatments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
    • Y10T428/139—Open-ended, self-supporting conduit, cylinder, or tube-type article
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
    • Y10T428/1397—Single layer [continuous layer]

Definitions

  • the present invention relates to a fine powder of a high molecular weight fluorine-based molten resin (particularly, this fine powder is used for a semiconductor jig, a jig of a process, etc.), a molded product obtained by molding this fine powder, and And a method for producing the same.
  • Fluorine-based molten resin is particularly excellent among various plastics. »It has chemical resistance, chemical resistance, electrical insulation, non-adhesiveness, and low friction properties. It is used in a wide range of fields, from industry to space development and aircraft industry to household goods.
  • fluorine-based molten resin has a higher melt viscosity, has a narrow range of suitable molding conditions, and decomposes slightly at high molding temperatures to generate corrosive gas. Is relatively difficult to mold.
  • those having a high molecular weight of 10 8 poise or higher have a too high melt viscosity and extremely low fluidity, so that it is extremely difficult to form them by ordinary extrusion or injection molding.
  • plastic generally has various advantages as the molecular weight decreases.
  • mechanical properties such as strength, elastic modulus, abrasion resistance and bending fatigue resistance
  • chemical properties such as weather resistance and chemical resistance. Therefore, naturally, it is expected that the above-mentioned very useful physical property improvement can be expected for the fluorine-based molten resin by increasing the molecular weight. Had not been converted.
  • technologies to reduce the molecular weight of fluoroplastics while maintaining mechanical and chemical properties have been studied.
  • the fluorine-based molten resin is usually molded by extrusion molding or injection molding. At this time, in order to improve the supply of raw materials to the molding machine such as hopper dropping and screw biteability, or to handle raw materials. It is provided as a pellet like other general-purpose plastics in order to facilitate the process.
  • the fluorine-based molten resin has the above-mentioned excellent characteristics, it is favorably used in the semiconductor manufacturing process as a molded article such as a wafer carrier, a tube, a joint, and a square tank.
  • a molded article such as a wafer carrier, a tube, a joint, and a square tank.
  • impurities such as particles and metals
  • Fluorine-based molten resin molded products used for this purpose have also been highly purified. Are increasing.
  • An object of the present invention is to improve the physical properties of a high-molecular-weight fluorine-based molten resin powder that has not been conventionally used, and to mold the fine powder to obtain a particle Molded products with reduced output, especially for semiconductor manufacturing processes, and these! ⁇ H is the way to go.
  • the present invention provides a melt viscosity of 10 ⁇ to 10 13 poise, an apparent density of 0.4 to 1.5 g / cc, and a specific surface area of 2 m 2 / g or less.
  • the present invention relates to a powder and a molded product obtained by molding the fine powder.
  • Examples of the type of the fluorine-based molten resin in the present invention include a copolymer of tetrafluoroethylene and a perfluoroalkylvinyl ether (hereinafter, referred to as PFA), tetrafluoroethylene and a hexafluorolob pen.
  • PFA perfluoroalkylvinyl ether
  • FEP a copolymer of tetrafluoroethylene and ethylene
  • ETFE a copolymer of tetrafluoroethylene and ethylene
  • PVDF a homopolymer of vinylidene fluoride
  • ECTFE a copolymer of ethylene and ethylene
  • m is an integer of 1 to 6.
  • CF 2 CF (0-CF 2 CF (CF A )) N OC 3 FT
  • n is an integer of 1 to 4
  • n is an integer of 1 to 4
  • n is an integer of 1 to 4
  • n is an integer of 1 to 4
  • n is an integer of 1 to 4
  • n is an integer of 1 to 4
  • FEP is preferably a copolymer of 72 to 96% by weight of tetrafluoroethylene and 4 to 28% by weight of hexafluoro ⁇ -propene
  • ETFE is a copolymer of 74.5 to 89.3% by weight of tetrafluoroethylene and 10.7 to 25.5% by weight of ethylene. Coalescence is preferred.
  • fluororesins may be those obtained by copolymerizing other monomers as copolymer components in an amount that does not impair the essential properties of each resin.
  • the melt viscosity of the fluorine-based molten resin in the present invention is indispensable to be 10 s to 10 13 poise from the viewpoint of reducing the amount of particles eluted and improving the quality of the molded product, and is preferably 10 6 to 10 1 ( ) Poise. What melt viscosity is less 10 6 pores Zuyori are those which are collectively referred to as fluorine-based molten resin commercially available-molding conventionally, it often also particles elution with low mechanical properties as described below Is not preferred.
  • those having a melt viscosity of more than 10 13 poise have to raise the molding processing temperature to a temperature higher than the thermal decomposition starting temperature of the resin in order to obtain a good molded product, and the molded product is foamed and colored, which is preferable. Absent.
  • the method for polymerizing the fluorine-based molten resin used in the present invention is not limited at all, and is produced by generally known emulsion polymerization, suspension polymerization, solution polymerization, block polymerization, or the like.
  • the apparent density of the fluorine-containing molten resin fine powder in the present invention is indispensable to be 0.4 to 1.5 g / cc from the viewpoint of powder flowability, moldability, and quality improvement of a molded product, Preferably, it is 0.5 to 1.4 g / cc. If the apparent density is less than 0.4 g / cc, the powder fluidity is poor, and the injection molding or molding tends to cause uneven filling in the mold, and a good molded product cannot be obtained. On the other hand, if the apparent density is higher than 1.5 g / cc, the powders are not sufficiently fused to each other, and a good molded product cannot be obtained.
  • the specific surface area of the fluorinated molten resin fine powder in the present invention is indispensable to be 2 mVg or less, preferably 1 mVg or less from the viewpoint of powder ⁇ property.
  • the specific surface area is larger than 2 m 2 / g, the powder fluidity is poor due to insufficient compaction of individual powders, and particularly in molding having a screw such as injection molding, the screw biting property is poor, which is preferable. Absent.
  • the average particle size is 10-2000 / zm, preferably 50-1000 zm.
  • the raw material powder of fluorinated molten resin (raw powder) after polymerization (after coagulation in the case of emulsion polymerization) has an apparent density of less than 0.4 g / cc and a specific surface roughness of more than 2 mVg.
  • the particles are not tight. Therefore, for the above reasons, this bulk powder cannot be used as it is in a molding machine, and it is necessary to increase the apparent density and reduce the specific surface area.
  • a high-molecular-weight fluorine-containing molten resin powder is passed through a roll to form a plate compressed at a lower ⁇ (at a melting point of -10), preferably at a pressure of 2 kg / cra 2 or more, and then pulverized. Can also be adopted.
  • a general pulverizer can be used, and it is not particularly limited, but a Henschel pulverizer, a rotor-one speed mill, and the like are particularly preferable.
  • a high molecular weight fluorine-based molten resin fine powder having an apparent density of 0.4 to 1.5 g / cc and a specific surface area of 2 raVg or less can be obtained.
  • the powder flowability is good and the raw material supply to the molding machine is good, and the following molding is possible.
  • the molding method according to the present invention can be carried out by slightly changing the conventional molding method, despite the fact that the fluorine-based molten resin used has the above-mentioned physical properties, such as compression molding, isostatic molding, and transfer molding. Molding methods such as molding, ram extrusion molding, extrusion molding, injection molding, blow molding, and flash flow molding can be applied.
  • the molding conditions differ depending on the molding method, but the molding temperature and mold temperature are higher by 10 to 60 ° C and the molding pressure is 50 to Preferably, it is 100 kg / cm 2 higher, the injection time and the injection time are slower by 10 to 100 sec, and the cooling time is longer by 50 to 100 sec.
  • the molding temperature thermal decomposition of the resin starts to prevent foaming and coloring of the molded product It must be:
  • a molded article having a desired shape can be obtained.
  • the molded article include a sheet, a film, a packing, a round bar, a square bar, a pipe, a tube, a ⁇ , a round tank, From simple molded products such as square tanks, tanks, etc., to complex shaped products such as wafer carriers, wafer boxes, bolts, beakers, filter housings, flow meters, pumps, valves, cocks, connection joints, connectors, nuts, etc. .
  • the molded article according to the present invention can be obtained by using a resin having a low molecular weight which has not been used conventionally. As a result, the proportion of low molecular weight substances in the resin has been relatively reduced. On the other hand, it has been pointed out that the main cause of the generation of particles eluted from fluorine-based molten resin molded products, which is a problem in the semiconductor manufacturing process, is that low-molecular-weight substances in the resin elute into the chemical solution. Therefore, the molded article according to the present invention has a small particle elution amount and is suitable for a semiconductor manufacturing process.
  • the high molecular weight fluororesin fine powder according to the present invention has a melt viscosity of 10 6 to 10 13 poise, an apparent density of 0.4 to: l. 5 g / cc, and a specific surface area of 2 mVg or less. Since it is a low molecular weight fluorine-based molten resin fine powder that has not been used, the molded product obtained from this fine powder has a reduced amount of particles eluted, and is particularly suitable for semiconductor manufacturing processes. Also, improvements in wear resistance and the like can be achieved.
  • thermogravimetric analyzer TGA-50, manufactured by Shimadzu Corporation
  • JI S K-1 6891 It is the value (g / cc) obtained by dropping the sample powder from a dumper into a stainless steel cylindrical container with an internal volume of 30 cc and scraping off the excess with a flat plate (g) divided by the internal volume (cc). .
  • MIT flex bending fatigue tester East Co., Ltd.
  • ⁇ Lfe pieces were cut out from 0.20 to 0.23 mm thick ffiig molded sheets.
  • the test conditions were as follows: a load of 1.25 kgf was applied, the bending speed was 178 times, and the bending angle was 135 °.
  • JISK-17204 Using a Taber abrasion tester (No.410, manufactured by Toyo Seiki Seisakusho), a compression molded sheet having a thickness of 1 mm and a diameter of 102 mra was measured as a test piece.
  • the test conditions were as follows: CS-10 was applied to the worn wheel, a load of 1 kgf was applied, and the wheel was worn 2000 times at a rotation speed of 70 rpm.
  • the Taber abrasion index was shown as the number of abrasion loss m m per 1000 times of abrasion.
  • a raw material PFA was filled into a cylinder having a nozzle via a hopper, and the temperature of the cylinder was raised to melt the PFA. Then, the molten fluororesin was injected into the cavity from the nozzle, and the fluororesin was compressed by applying a compression pressure of 30 kgf / cm 2 using the SJf & plate.
  • the raw materials used in this molding had good hopper dropping, good screw biting properties, and could be molded with stable weighing.
  • the molded product obtained is free of foaming and coloring, free of insufficient fusion and whitening due to insufficient fusion, and is good and o
  • Comparative Example 1 using commercially available PF A pellets with a melt viscosity of 2.5 ⁇ 10 5 poise Perform injection molding using the same injection molding machine and molding conditions as shown in Table 1 below./o
  • This raw material had good hopper removal, good screw penetration, and could be molded with stable weighing.
  • the obtained molded product was good without foaming or coloring, and without whitening due to insufficient fusion or insufficient fusion.
  • DHP 6, 6, 7, 7-dodecafluoroheptanyl peroxide
  • the white powder produced in the autoclave was washed with water and dried at 120 ° C. for 12 hours to obtain 270 parts of the desired high molecular weight PFA powder.
  • the physical properties of this PFA were a melt viscosity of 4.2 ⁇ 10 6 poise and a PPVE composition of 3.2% by weight (measured by melt NMR measurement). Other physical properties are as shown in Table 1 below.
  • injection molding was attempted using the same injection molding machine as in Comparative Example 1 under the molding conditions shown in Table 1 below. However, it was difficult to charge the material because the raw material was idle at a part of the screw. In addition, charging was performed by sticking with a stick from the hopper, but the measurement was unstable, and a good molded product could not be obtained.
  • the high molecular weight PFA powder obtained in Comparative Example 3 was heated in an electric furnace at 310 at 6 hours, and then pulverized for 10 minutes by a Hensile mill.
  • the physical properties of the obtained low molecular weight PFA fine powder were as shown in Table 1 below.
  • the obtained sheet-like molded product was good without foaming or coloring, and without whitening due to insufficient fusion or insufficient fusion.
  • the obtained sheet-like molded product was good without foaming or coloring, and without whitening due to insufficient fusion or insufficient fusion.
  • HFP hexafluoropropene
  • the white powder produced in the autoclave was washed with water and dried at 120 for 12 hours to obtain 415 parts of the target ultrahigh molecular weight FEP powder.
  • the physical properties of this FEP were a melt viscosity of 2.9 ⁇ 10 6 bores and an HFP composition of 8.2% by weight (measured by melt NMR). Other physical properties are as shown in Table 2 below.
  • the high molecular weight FEP powder obtained in Comparative Example 6 was After hardening into a plate at room temperature at ⁇ -rpm of 0.4 rpm using a model GBS manufactured by Higashi Kogyo Co., Ltd., it was pulverized by a crusher at 360 rpm.
  • the physical properties of the obtained low molecular weight FEP fine powder were as shown in Table 2 below.
  • the obtained sheet-like molded product was good without foaming or coloring, and without whitening due to insufficient fusion or insufficient fusion.
  • the obtained sheet-shaped molded product was good without foaming or coloring, and without whitening due to insufficient fusion or insufficient fusion.
  • the obtained sheet-shaped molded product was whitened due to insufficient fusion or insufficient fusion, and its surface was rough, making it impractical.
  • the high molecular weight ETFE powder obtained in Comparative Example 9 was heated in an electric furnace at 255 ° C. for 4 hours, and then pulverized with a Henschel pulverizer for 10 minutes.
  • the resulting polymer The physical properties of the ETFE fine powder were as shown in Table 3 below.
  • dumbbells were punched out, and a particle elution test was performed using these as samples.
  • a dumbbell type 5 described in ASTM D 638 was used. These dumbbells were contaminated by the atmosphere during the molding and punching processes, and had significant particles attached to their surfaces.To remove these, pre-cleaning was performed in the following procedure. .
  • the dumbbells Rinse the dumbbells with ultrapure water for 5 minutes, place in a clean polyethylene bottle with an internal volume of 11 and add 200 g of 50% hydrofluoric acid of high ⁇ K grade for semiconductors to the shaker. For 5 minutes. After standing for 24 hours, the hydrofluoric acid was discarded and rinsed with ultrapure water for 5 minutes. Subsequently, the dumbbell was immersed in 100 ml of a low-grade sulfuric acid / hydrogen peroxide mixed solution for semiconductors (volume ratio: 4: 1) for 5 minutes, and further rinsed with ultrapure water for 5 minutes.
  • dumbbells Put each of the five pre-cleaned dumbbells into a clean polyethylene bottle with an internal volume of 11 and add 200 g of low-grade 50% hydrofluoric acid for semiconductors to the bottle. Shake for a minute.
  • the particles (0.2 m or more) in the hydrofluoric acid were measured using a particle counter (KL-22, manufactured by RION).
  • the measurement results of the elution particles are shown in Table 4 below.
  • Table 4 shows the values measured under the same conditions without dumbbells as a reference example. Examples 1-3 As for the dumbbell made of fluorine resin of low molecular weight, the particle elution amount was significantly small.
  • Example 3 Commercially available ⁇ molecular weight ⁇ molecular weight Low viscosity High viscosity Melt viscosity Poise 2.2X10 4 4.6X10 4 6.0X10 6 6.0X10 6 original " ⁇ , At 266 265 265 265 pyrolysis
  • the molded article of the high molecular weight fluorine-based resin fine powder according to the present invention is excellent in bending fatigue resistance and wear resistance, and in particular, the particle elution amount is reduced by half compared to the conventional product. Suitable for semiconductor manufacturing process applications.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

Une poudre fine de fluororésine fondue, de masse moléculaire élevée, présente une viscosité de fusion de 10?8 à 1013¿ P, une densité apparente de 0,4 à 1,5 g/cm3 et une surface spécifique égale ou inférieure à 2 m2/g. Un article moulé fabriqué à partir de cette fluororésine, qui n'a pas été utilisée jusqu'ici, présente une fuite réduite de particules, peut être en particulier utilisé dans un procédé de fabrication de semi-conducteurs, et peut notamment avoir une meilleure résistance à la fatigue en flexion et une meilleure résistance à l'usure.
PCT/JP1995/001423 1994-07-22 1995-07-17 Poudre fine de fluororesine fondue, de masse moleculaire elevee, article moule obtenu et leur procede de production WO1996003446A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE69530927T DE69530927T2 (de) 1994-07-22 1995-07-17 yEINES PULVER AUS GESCHMOLZENEM HOCHMOLEKULAREM FLUORHARZ, DARAUS GEFORMTER GEGENSTAND UND VERFAHREN ZU DEREN HERTSTELLUNG
US08/765,454 US6365243B1 (en) 1994-07-22 1995-07-17 Fine powder of high molecular weight fluorine containing fused resins, its mold goods, and the dedicated production methods
EP95925140A EP0773244B1 (fr) 1994-07-22 1995-07-17 Poudre fine de fluororesine fondue, de masse moleculaire elevee, article moule obtenu et leur procede de production

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP19183794A JP3671435B2 (ja) 1994-07-22 1994-07-22 高分子量フッ素系溶融樹脂微粉末、その成形品、及びこれらの製造方法
JP6/191837 1994-07-22

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WO1996003446A1 true WO1996003446A1 (fr) 1996-02-08

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US (1) US6365243B1 (fr)
EP (1) EP0773244B1 (fr)
JP (1) JP3671435B2 (fr)
DE (1) DE69530927T2 (fr)
WO (1) WO1996003446A1 (fr)

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WO1997040089A1 (fr) * 1996-04-24 1997-10-30 Daikin Industries, Ltd. Fluoropolymere en poudre et procede de preparation
JP4618911B2 (ja) * 2001-03-09 2011-01-26 倉敷紡績株式会社 Ｐｆａ樹脂の改良方法
JP4894096B2 (ja) * 2001-06-18 2012-03-07 ダイキン工業株式会社 フッ素系重合体粉末製造方法
US20030109646A1 (en) * 2001-11-21 2003-06-12 Daikin Institute Of Advanced Chemistry And Technology Resin composition and method of producing shaped articles
US6870020B2 (en) * 2002-04-30 2005-03-22 E. I. Du Pont De Nemours And Company High vinyl ether modified sinterable polytetrafluoroethylene
EP1643818A4 (fr) * 2003-07-03 2006-08-16 Hitachi Ltd Module et procede de fabrication de celui-ci
WO2011052666A1 (fr) * 2009-10-30 2011-05-05 株式会社クレハ Poudre de polymère de fluorure de vinylidène et solution de polymère de fluorure de vinylidène
CN103764728A (zh) * 2011-08-29 2014-04-30 大金工业株式会社 含氟聚合物粉末、覆膜以及含氟聚合物粉末的制造方法
WO2017069069A1 (fr) * 2015-10-20 2017-04-27 旭硝子株式会社 Résine fluorée et son procédé de production
JP7044673B2 (ja) * 2018-09-11 2022-03-30 株式会社クレハ フッ化ビニリデン系ポリマー粉末、バインダー組成物、電極合剤、および電極の製造方法
JP7339830B2 (ja) * 2018-09-28 2023-09-06 東ソー株式会社 フッ素樹脂粒子およびその製造方法
CN117447634A (zh) 2018-09-28 2024-01-26 东曹株式会社 氟树脂、氟树脂粒子及它们的制造方法
WO2020075724A1 (fr) 2018-10-09 2020-04-16 東ソ－株式会社 Résine fluorée, son procédé de production, et procédé de production de particules de résine fluorée
JP7295507B2 (ja) * 2019-03-27 2023-06-21 東ソー株式会社 フッ素樹脂の製造方法

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Also Published As

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JPH0834820A (ja) 1996-02-06
DE69530927D1 (de) 2003-07-03
EP0773244A4 (fr) 1997-11-19
US6365243B1 (en) 2002-04-02
DE69530927T2 (de) 2004-05-19
EP0773244B1 (fr) 2003-05-28
EP0773244A1 (fr) 1997-05-14
JP3671435B2 (ja) 2005-07-13

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